GC-ECD를 이용한 배추, 사과, 감귤, 고추, 현미 중 살균제 Prochloraz의 분석법 확립 = Establishment of Analytical Method of Prochloraz in Cabbage, Apple, Mandarin, Pepper and Hulled rice with GC-ECD

국문 초록 (Abstract)

Prochloraz를 2,4,6-Trichlorophenol (2,4,6-TCP)로 전환시켜 분석하는 방법을 확립하였으며, 배추, 사과, 고추. 감귤, 현미를 대사 농작물로 선정하였다. 농산물 시료를 마쇄, acetonitrile로 추출하여 dichloromethane으로 분배하고 농축액에 pyridine hydrochloride를 넣고 1시간 가열 분해를 한다. 반응액을 다시 dichloromethane으로 분배한 후 GC-ECD로 분석하였다. Prochloraz의 정량한계는 0.01 mg/kg 이었다. 회수율은 0.1 mg/kg 수준에서 105-113%, 0.5 mg/kg 수준에서 82-87% 이었고, 반복 간 분석오차는 10% 미만이었다. 이러한 분석법 개선 과정에서 기존의 soxhlet 추출과 환류장치를 쓰지 않고 용매추출법과 작은 vial을 성공적으로 적용하였고, 간편, 신속, 경제적이며 정밀한 분석법을 확립하였다.

다국어 초록 (Multilingual Abstract)

Analytical method for prochloraz in cabbage, apple, pepper, mandarin, and hulled rice was established by conversion it to 2,4,6-trichlorophenol (TCP). Crop samples were extracted with acetonitrile, and partitioned with dichloromethane. The sample extracts were hydrolyzed with pyridine hydrochloride in a vial by heating for 1 hour, and analyzed with GC-ECD after partitioning with dichloromethane. Method quantification limit (MQL) of prochloraz was 0.01 mg/kg. Recoveries at 0.1 mg/kg level was 105-113% while at 0.5 mg/kg level was 82-87%. In both of the cases CV was less than 10%. Through this procedure soxhlet extraction and refluxing apparatus of conventional method were discarded and simple solvent extraction and small vial were successfully employed, resulting in simple, rapid, economic and more precise method.

참고문헌 (Reference)

1 Hollrial-Rosta A, 55 : 531-538, 1999

2 이종화, "시설 내 오이 재배 중 살균제 Boscalid의 잔류특성" 한국농약과학회 12 (12): 67-73, 2008

3 Rood, Dean, "The Troubleshooting and Maintenance Guide for Gas Chromatographers" Wiley-VCH 16-17, 2007

4 Tomlin, C. D. S, "The Pesticide Manual (14th)"

5 De Paoli M., "Simpligied determination of combine resides of prochloraz and its metabolites in vegetable, fruit and wheat samples by gas chromatography" 765 : 127-131, 1997

6 Daniel C. Harris, "Quantitative chemical analysis (3rd)" W. H. Freeman and company 450-, 1997

7 "Pesticide analytical method" Chungang Press 714-, 2006

8 Fong, W. G, "Pesticide Residues in food: Methods, Technologies, and Regulations" Wiley Interscience 3-44, 1999

9 Korea crop protection associa, "Pesticide Field Manual" Samjeong Press 2009

10 최용화, "Imidazole계 살균제 Prochloraz의 토양 중 잔류량과 반감기분석" 한국분석과학회 15 (15): 10-71, 2002

11 Miller, J. M, "Chromatography : concepts and contrasts (2nd)" Wiley Intersciense 286-287, 2005

12 Bienvendia, G, "British Crop Production Council, UKBienvenida Determination of Postharvest Fungicides in Fruit Juices by Solid-Phase Extraction Followed by Liquid Chromatography Electrospray Time-of-Flight Mass Spectrometry" 55 : 10548-10556, 2007

13 McNair, H. M, "Basic Gas Chromatography" Wiley Interscience 7-51, 1997

14 Sandro, N, "An alternative LC-UV Procedure for the determination of Prochloraz residue in fruits" 16 : 157-162, 2005